Coloration of textile material



Patented Jan. 3, 1933 UNITED STATES PATENT OFFICE ALBERT MELLOR AN'DDAVID MCLELLAN, OF SPONDON, NEAR DERBY, ENGLAND,

ASSIGNORS TO CELANESE CORPORATION OF AMERICA, A CORPORATION OF DELA-WARE COLORATION OF TEXTILE MATERIAL No Drawing. Application filedJanuary 29, 1931, Serial No. 512,212, and in Great Britain April 2,1930.-

This invention relates to the production of uniform black colorations onmixed materials containing derivatives of cellulose and vegetable orother textile fibres.

A very widely used method for the production of black colorations ontextile bres 1s the oxidation of aniline on the material. By this meansthere may be very cheaply produced excellent blacks of exceptionalfastness.

Considerable difiiculties have, however, been encountered in theproduction of uniform aniline black shades on mixed materials containingcellulose derivatives and vegetable, animal or other textile fibres,since, in general, the conditions necessary for the production of thebest blacks on the cellulose derivative on the one hand and on thecellulosic or animal fibres on the other hand are not identical. Thusfor example in addition to the different affinities of cellulose acetateand cotton for aniline, the conditions for the oxidation of aniline to agood black on cotton are very difierent from the conditions required forthe production of a good black on cellulose acetate.

According to the present invention uniform black colorations areobtained on mixed materials containing derivatives of cellulose andother textile fibres by first causing the mixed material to absorbpara-aminodiphenylamine or a derivative thereof, and then mechanicallyimpregnating it with aniline or its homologues or compounds thereof andoxidizing.

By such a process the para-aminodiphenylamine or the like ispreferentially absorbed substantively by the cellulose derivative, whileboth or all the constituents of the mixed materials are impregnated withaniline or the like.

The diphenylamine base may be absorbed substantively from solution ordispersion. Advantageously solutions may, prior to application, be madeacid by means of suitable acids, preferably organic acids, e. g. lacticacid or acetic acid. The substantive treatment is preferably givenhowever, with the diphenylamine base in dispersion. Thus for example themixed fabric may be immersed dried, aged, and if desired, chromed, orsubjected to any other desired after-treatment.

If desired, instead of applying to the material the diphenylamine basethe latter may be produced on the material. Thus for example 2-l-dinitrodiphenylamine or other p-nitrodiphenylamine may be applied tothe mixed material and then reduced on the material to give the aminobody.

The absorption of the diphenylamine base or other diphenylamine body andthe compound of aniline or homologues of aniline into the cellulosederivative fibre may be promoted by means of alcohol, hydroquinone, orother substance having a swelling action on the fibre. The oxidizingagent or mixture employed for the production of a black may contain achlorate, hypochlorite, bichromate, or other suitable oxidizing agent,and may also contain one or more catalysts or oxygen carriers, e. g.salts of vanadium, copper, iron or chromium. The development of thecolor may also be assisted by means of aluminium chloride or any othersuitable inorganic assistant.

The following example illustrates carrying the invention into effect,but it is to be understood that it is in no Way limitative 100 pounds ofa mixed fabric containing cotton and cellulose acetate are scoured at C.on a-dye' jig in a 30 to 1 bath containing 1 gram'per litre of soap and2 cos. per litre Turkey red oil. After'half an hour 10 pounds of a 10per cent. dispersion of para-aminodiphenylamine in Turkey red oil isadded to the scouring bath, and the fabric treated for a further half anhour at 80 to, 85 0.; at the close of this period the fabric me p iswashed in warm water, hydroextracted and dried. It is then padded in. ananiline liquor made up as follows 84 pounds aniline hydrochloride, 18pounds potassium chlorate, 18 pounds crystallized copper sulphate, waterto make 80 gallons. The material is finally dried, aged at 45 to 50 C.and chromed with 1 to 3 Tw. sodium bichromate at ordinary temperaturesfor one hour. An excellent uniform black is thus obtained on the matcriaThe process of the present invention aims more particularly at producinguniform blacks on mixed materials comprising a cellulose derivative andcotton, linen, regenerated cellulose, artificial silks or rayons, orother cellulosic fibres. It is however of considerable use in theproduction of un form blacks on mixed materials comprising cellulosederivatives and animal fibres, for example, natural silk. The mixedmaterial may contain any organic derivative. of cellulose. Thus forexample the material may contain cellulose acetate as already mentioned,or it may contain other organic esters of cellulose, e. g. celluloseformate, propionate, butyrate, or the products obtainable by thetreatment of alkalized cellulose with an esterifying agent, e. g. theproduct known an immunized cotton obtained by treating alkalizedcellulose with para-toluene sulphochloride. Again, the material maycontain cellulose ethers, for example methyl, ethyl or benzyl celluloseor'the correspond ng condensation products of cellulose and glycols, orother polyhydric alcohols.

at we claim and desire to secure by Letters Patent is 1. Process for theproduction of black colcomprising causing the cellulose derivatives toabsorb a compound selected from the group consisting ofpara-aminodiphenylamine and its derivatives, mechanically impregnatingthe mixed material with a substance selected from the group consistingof aniline, its homologues, and its compounds, and subjecting thematerial to theaction of an oxidizing agent.

2. Process for the production of black colorations on mixed materialscontaining cellulose acetate and cellulosic fibres, comprising causingthe cellulose acetate to absorb a compound selected from the groupconsisting of para-aminodiphenylamine and its derivatives, mechanicallyimpregnating the mixed material with a substance selected from the groupconsisting of aniline, its homologues, and its compounds, and subjectingthe material to the action of an oxidizing agent.

3. Process for the production of black colorations on mixed materialscontaining cellulose acetate and cotton, comprising causing thecellulose acetate to absorb a compound absorb a compound of the groupconsisting K of para-aminodiphenylamine and its derivatlves from anaqueous dispersion of sand compound, mechanically impregnating the mixedmaterial with a compound selected from the group consisting of aniline,its homologues, and its compounds, and subjecting the materials to theaction of an oxidizing agent.

5. Process for the production of black colorations on mixed materialscontaining cellulose acetate and cellulosic fibres comprising causingthe cellulose acetate to absorb a compound of the group consisting ofpara-aminodiphenylamine and its derivatives from an aqueous dispersionof said compound, mechanically impregnating the mixed material with acompound selected from the group consisting of aniline, its homologuesand its compounds, and subjecting the material to the action of anoxidizing agent.

, 6. Process for the production of black colorations on mixed materialscontaining derivatives of cellulose and cellulosic fibres, comprisingproducing on the cellulose derivative fibre a para-aminodiphenylamine byreduction of the corresponding nitro compound, mechanically impregnatingthe mixed material with a compound selected from the group consisting ofaniline, its homologues. and its compounds, and subjecting the materialto the action of an oxidizing agent.

In testimony whereof we have hereunto subscribed our names;

ALBERT MELLOR. DAVID TELFER MoLELLAN.

